Ingenieurwissenschaften und zugeordnete Tätigkeiten
Filtern
Dokumenttyp
- Zeitschriftenartikel (6)
- Posterpräsentation (5)
- Vortrag (4)
- Beitrag zu einem Tagungsband (1)
Schlagworte
- FTIR (16) (entfernen)
Organisationseinheit der BAM
- 7 Bauwerkssicherheit (5)
- 7.1 Baustoffe (4)
- 3 Gefahrgutumschließungen; Energiespeicher (3)
- 6 Materialchemie (3)
- 1 Analytische Chemie; Referenzmaterialien (2)
- 3.2 Gefahrguttanks und Unfallmechanik (2)
- 4 Material und Umwelt (2)
- 4.5 Kunst- und Kulturgutanalyse (2)
- 6.3 Strukturanalytik (2)
- 1.2 Biophotonik (1)
Eingeladener Vortrag
- nein (4)
Heizöllagerbehälter aus Polyethylenformstoffen werden seit Beginn der 70-iger Jahre in Deutschland hergestellt. Die Hersteller empfehlen zur Gewährleistung der Sicherheit nach Ablauf von 30 Jahren den Ersatz dieser Behälter. Polyethylenformstoffe unterliegen im Laufe ihrer Nutzungsdauer der Alterung durch die Veränderung ihrer Eigenschaften. Das Ausmaß der Alterung und die Art des Abbauvorganges hängen im Wesentlichen vom chemischen Abbau des Polyethylens, der Wanddicke des Behälters und den Umgebungsbedingungen ab. Bisher lagen keine Untersuchungen zum Langzeitverhalten der Polyethylenformstoffe vor, insbesondere nach einer Nutzungsdauer der Tanks über 30 Jahre. Ziel der Untersu-chungen war, den tatsächlichen Schädigungsgrad der Polyethylenformstoffe im Vergleich zu den unbelasteten Formstoffen zu ermitteln. Da die BAM bis Mitte der 90-iger Jahre für die Prüfungen und Gutachten zur Zulassung dieser Behälter zuständig war, sind die Werkstoffdaten noch vorhanden.
Als Untersuchungsmethoden wurden die Bestimmung der Schmelze-Masse-Fließrate (MFR) und die Fourier-Transformation-IR-Spektroskopie (FTIR) von Tankausschnitten aus dem Bereich des Bodens, des Mantels und des Daches von 10 ausgesonderten Behältern aus den Polyethylenformstoffen A und B herangezogen. Die Messungen der MFR der Tankaus-schnitte aus diesen Bereichen zeigten Unterschiede in den Werten in Abhängigkeit vom Ge-wicht (5 kg oder 21,6 kg), welches eingesetzt wurde. Eine Abnahme der MFR-Werte wurde für die größere Anzahl der Tankwandungsausschnitte aus dem Formstoff B nach einer Lebensdauer der Tanks > 30 Jahre gemessen. Dieser Formstoff wurde hauptsächlich durch innere Alterung infolge Vernetzungen, Verzweigungen und Weichmacherverlust und weniger durch oxidativen Abbau geschädigt. Die FTIR-Messungen der Proben aus dem Bereich des Bodens und des Mantels der Tanks zeigten, dass die Intensität der asymmetrischen/symmetrischen CH2 -Streckschwingungen im Bereich: 2800 - 2900 cm-1 und der CH2 -Biegeverformungsschwingung bei 1400 cm-1 aufgrund von Kettenspaltungen zugenommen haben. Die Intensität der Carbonylstreckschwingung C=O bei 1740 cm-1 ist niedrig. Sie ist ein Maß für die Oxidation des Polymerwerkstoffes.
In der Berliner Sammlung "Manuscripta Americana" befinden sich Fragmente von Bilderhandschriften, die Alexander von Humboldt 1804 in Mexiko erwarb und der Königlichen Bibliothek schenkte. Die in der frühen Kolonialzeit hergestellten verschiedenartigen Codices waren damals schon nicht mehr an den Orten ihrer ursprünglichen Verwendung. Entsprechend ihres Seltenheitswertes gelangten einzelne Schriftstücke seit der Conquista in die Bestände bedeutender Persönlichkeiten. Hierzu fertigte man auch Abschriften oder Kopien an, oder zerstückelte sogar einzelne Blätter, so dass die Darstellungen auf den abgetrennten Fragmenten oft nur zum Teil abgebildet vorliegen.
Um herauszufinden, ob einige Schriftstücke der "Humboldt Codices" in Bezug zu einander stehen, werden die Dokumente, ihre Symbole und Schriftzeichen und das zur Herstellung verwendete Material miteinander verglichen.
Mit den für die Analyse von Manuskripten bewährten Untersuchungsmethoden werden Papier und Farbmittel identifiziert. Hierzu zählen Raman-, FTIR-, Röntgenfluoreszenz- und VIS- Spektroskopie. Charakteristisch für die Herstellung von schriftlichen Dokumenten in der Kolonialzeit von Amerika ist die Verwendung von indigenem Material wie Papier aus Baumrinde und Pflanzenfarben zusammen mit den aus Europa bekannten Materialien. Geklärt wird, inwieweit neben den bekanntesten Farbstoffen wie Cochenille, Mayablau oder Mischungen mit Tonmineralen auch mineralische Pigmente zum Einsatz kamen.
Vorgestellt werden die auf Tafel 36 in den "Vues des Cordillères et Monuments des Peuples Indigènes de l`Amerique, Voyage de Humboldt et Bonpland" abgebildeten Fragmente. Die hier von Humboldt vorgenommene Zusammenstellung wird mit der Farbpalette der in Berlin archivierten originalen Schriftstücke verglichen. Die Interpretation der Ergebnisse gibt einen Hinweis auf die Zuordnung oder auch Zusammengehörigkeit dieser einzigartigen Dokumente amerikanischer Geschichte. Hierbei wird die Frage aufgeworfen, inwiefern davon auszugehen ist, dass diese mit weiteren Fragmenten in Verbindung gebracht werden können, was für die Beleuchtung der kulturhistorischen Zusammenhänge von großer Bedeutung ist.
In Germany, the reuse of asphalt has a long tradition. Since the 1980s, the reclaimed asphalt has been recycled achieving a reuse rate of around 90% and thus a very high value in the last years. In the future, instead of the amount, the quality of the reclaimed asphalt will be more important because the recycled asphalt will be reused again and again. Thus, these asphalt mixes are in the second or even third cycle of reuse. Concerning this situation, the question arises if asphalt can be reused several times without any loss in quality. An important factor affecting the asphalt quality is the binder bitumen. During the production, construction and service life, the ageing of this binder occurs causing a hardening of the bitumen. To compensate this hardening, additives for the reclaimed asphalt in terms of rejuvenation agents (rejuvenators) gain in importance. With these rejuvenators, the physical properties of bitumen can be modified e.g. the hardness and the stiffness reduced. However, the mechanism of the rejuvenation agents and the effects of the bitumen chemistry are largely unknown because the composition of the products varies very strongly. But with growing knowledge about these mechanisms and effects of the rejuvenation agents, the chemical composition and thus the physical and ageing behavior of bitumen can be targeted modified by the use of suitable rejuvenators. In this work, the actual results of the project Postcarbone road should be presented including investigations about the chemical and physical mechanisms as well as the efficiency of different rejuvenators.
Further, a model for the cyclic reuse of bitumen should be developed. Based on this model, the choice of a suitable rejuvenation agent for the considered bitumen or rather asphalt should be possible. The project Postcarbone road (392670763) is funded by the German Research Foundation (DFG).
In Germany, the reuse of asphalt has a long tradition. Since the 1980s, the reclaimed
asphalt has been recycled achieving a reuse rate of around 90% and thus a very high
value in the last years. In the future, instead of the amount, the quality of the
reclaimed asphalt will be more important because the recycled asphalt will be reused
again and again. Thus, these asphalt mixes are in the second or even third cycle of
reuse. Concerning this situation, the question arises if asphalt can be reused several
times without any loss in quality. An important factor affecting the asphalt quality is the
binder bitumen. During the production, construction and service life, the ageing of this
binder occurs causing a hardening of the bitumen. To compensate this hardening,
additives for the reclaimed asphalt in terms of rejuvenation agents (rejuvenators) gain
in importance. With these rejuvenators, the physical properties of bitumen can be
modified e.g. the hardness and the stiffness reduced. However, the mechanism of the
rejuvenation agents and the effects of the bitumen chemistry are largely unknown
because the composition of the products varies very strongly. But with growing
knowledge about these mechanisms and effects of the rejuvenation agents, the
chemical composition and thus the physical and ageing behavior of bitumen can be
targeted modified by the use of suitable rejuvenators. In this work, the actual results of
the project Postcarbone road should be presented including investigations about the
chemical and physical mechanisms as well as the efficiency of different rejuvenators.
Further, a model for the cyclic reuse of bitumen should be developed. Based on this
model, the choice of a suitable rejuvenation agent for the considered bitumen or rather
asphalt should be possible. The project Postcarbone road (392670763) is funded by the
German Research Foundation (DFG).
Casks for storage and transportation of used fuel rods of radioactive material are equipped with polyethylene (PE) for improved neutron flux shielding. The embedded PE structures are additionally exposed to gamma radiation and heat flow due to the specific high activity of the fission products. 60Co γ-radiation and heat load experiments at 125°C has been performed to evaluate PE degradation during the ageing process. FAR-FTIR-experiments were subsequently performed at differently aged PE test samples to characterize the oxidation process and morphological changes in the samples during the ageing at 125°C.
New Focus On Boehmite-Reinforced Nanocomposites Molecular Approach With Advanced FTIR-Techniques
(2019)
By FTIR-study it was possible to proof a chemical reaction between boehmite and the hardener of anhydride cured epoxy resins. Future studies can assume that the chemical environment of the resin system is changed in the surrounding of boehmite nanoparticles. This highly affects especially localized properties.
Clays are crucial mineral phases in Earth’s weathering engine, but we do not know how they form in surface environments under (near-)ambient pressures and temperatures. Most synthesis routes, attempting to give insights into the plausible mechanisms, rely on hydrothermal conditions, yet many geological studies showed that clays may actually form at moderate temperatures (<100 °C) in most terrestrial settings. Here, we combined high-energy X-ray diffraction, infrared spectroscopy, and transmission electron microscopy to derive the mechanistic pathways of the low-temperature (25–95 °C) crystallization of a synthetic Mg-clay, saponite. Our results reveal that saponite crystallizes via a two stage process: (1) a rapid (several minutes) coprecipitation where ∼20% of the available magnesium becomes incorporated into an aluminosilicate network, followed by (2) a much slower crystallization mechanism (several hours to days) where the remaining magnesium becomes gradually incorporated into the growing saponite sheet structure.
Tanks for heating oil made of polyethylene grades have been on the market since the early 1970s in Germany. Tank manufacturers recommend the replacement of the tanks after a period of 30 years due to guarantee safety. Polyethylene grades are subject to ageing by alteration of the properties during their life cycle. The degree of ageing and the nature of the degradation process mainly depend on the chemical degradation of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no results available on the long-term behavior of the polyethylene grades, especially after a service life of more than 30 years. The aim of this investigation was the determination of the factual degree of damage in comparison to the uncontaminated polyethylene grades. Material data of the used polyethylene grades are available because the BAM was the competent authority for the tests and expert reports for the approval of these tanks until the middle of the 1990s.
The determination of the Melt Flow Rate (MFR) and the Fourier Transmission IR Spectroscopy (FTIR) of tank sections from the bottom, the shell and the roof of 10 segregated heating oil storage tanks produced of polyethylene grades A and B were used as tests methods.
The MFR measurements of the tank sections showed differences in the values depending on the weight which was used (5 kg or 21.6 kg). A reduction of the MFR values was measured for most of the sections of tanks made of polyethylene grade B after a service life of the tanks of more than 30 years. This grade is mainly subject to the internal ageing by cross-linkages, increased degree of branched molecules and loss of the plasticizer, and to a lesser extent by oxidative degradation. The FTIR analysis, especially of tank sections of the bottom and the shell showed that the intensity of the CH2 asymmetric and symmetric stretching vibrations in the range: 2800 - 2900 cm-1 and the CH2 bending deformation vibration at 1400 cm-1 increased due chain scissions. The intensity of the carbonyl stretching vibration C=O at 1740 cm-1 is low. The carbonyl index characterizes the degree of oxidation.
Das erdölstammige Bindemittel Bitumen weist eine so komplexe Struktur auf, dass diese mit den derzeit eingesetzten Verfahren nur eingeschränkt erfasst werden kann. Eine innovative und vielversprechende Möglichkeit bietet in diesem Zusammenhang die FTIR-Spektroskopie in Kombination mit einer chemometrischen Auswertung, mit der schnell und einfach Aussagen über die Zusammensetzung sowie verschiedenste physikalische und chemische Eigenschaften von bitumenhaltigen Materialien möglich werden.
In this work, a methodology based on Fourier transform infrared (FTIR)spectroscopy and multivariate evaluation is presented to estimate the aging sensitivity of bitumen based on the unaged samples and thus without the need for time- and material-consuming aging simulations. For this purpose, factor analysis and linear discriminant analysis are used to develop a statistical model based on the FTIR spectra of unaged bitumen samples, which can be used fast and simple in everyday laboratory work and allows to assign the bitumen to a low, moderate, or strong aging sensitivity. The evaluation of the aging sensitivity is based on the complex shear modulus|G* | and the phase angle δ from the measurement with a dynamic shear rheometer(DSR), whose aging-related changes were captured as the slope in the Black diagram. A relevant influence on the classification concerning the aging sensitivity has the oxygen-containing compounds(sulfoxide, hydroxyl and partly carbonyl compounds), whereby lower contents and thus less preaged bitumen tend to have a stronger aging sensitivity. However, in addition to the oxygen-containing compounds, the structure of the aliphatic and aromatic compounds and, in particular, the interaction of the different structures are decisive for the aging sensitivity
We report the synthesis and characterization of carbon nanodots (CDs) with high quantum yield (>50%) and tailored optical absorption as well as emission properties. A well-described protocol with polyethyleneimine (PEI) as amine precursor is used as a reference to a new CD system which is stabilized by aromatic 2,3-diaminopyridine (DAP) molecules instead. The DAP stabilizer is installed in order to red-shift the absorption peak of the n-π* electron transition allowing efficient radiative recombination and light emission. Size, shape, and chemical composition of the samples are determined by (HR)TEM, EDX and FTIR-spectroscopy. Optical parameters are investigated using UV-VIS, PL and QY measurements. Several parameters such as concentration, excitation wavelength and pH are studied. Zeta-potential analysis indicate that pH-induced (de-)protonation processes of functional moieties directly affect the n-π* energy bands. This results in unique pH-dependent absorption and emission characteristics which are discussed on the specific chemical composition of each CD system.
Copolymers made of polycarbonate (PC) and polydimethylsiloxane (PDMS) are broadly applied in material science. High impact-stability and transparency are the marks of bisphenol-A polycarbonate. PDMS on the other hand excels in thermal stability, flame resistance and weatherability. Combining those favourable characteristics in a copolymer yields in a ductile but impact-resistant and flame retardant material. In order to understand the synthesis process and to improve the quality and characteristics of a copolymer, knowing its structure is essential. The challenge lies in the variety of heterogeneities like molecular mass-, block-size- and block-distribution.
This study addresses the structural characterization of PC-PDMS-copolymers using different liquid chromatographic techniques, including two dimensional combinations, hyphenated to MALDI-mass spectrometry and FTIR. The large difference in polarities of PC and PDMS is a challenge for liquid chromatography as well as ionization in MALDI. Nevertheless, we were able to differentiate between homopolymer and actual copolymer, clarify the presence of cyclic structures and gain information about the PDMS blocks
The structure and composition of polycarbonate polydimethylsiloxane copolymer (PC-co-PDMS) was investigated by applying various analytical approaches including chromatographic separation methods, spectrometric, and spectroscopic detection techniques. In particular, size exclusion chromatography (SEC) and liquid adsorption chromatography operating at different conditions (e.g. using gradient solvent systems) were used to achieve separations according to molar mass and functionality distribution. The coupling of both techniques resulted in fingerprint two-dimensional plots, which could be used to easily compare different copolymer batches. Matrix-assisted laser desorption/ionization-time-of-flight (MALDI-TOF) mass spectrometry was applied for structural investigations. The different ionization behavior of both comonomers, however, strongly limited the applicability of this technique. In contrast to that, Fourier-transform Infrared (FTIR) spectroscopy could be used to quantify the amount of PDMS in the copolymer at different points in the chromatogram. The resulting methodology was capable of distinguishing PC-co-PDMS copolymer from PC homopolymer chains present in the material.
The mayor part of the Berlin collection `Manuscripta Americana´ consists of documents compiled by Alexander von Humboldt. The diversity of the written fragments and their shape presume few accordance concerning purpose, place or time of production. Even before the papers came to Berlin, manuscripts were copied, divided and collected by famous scholars also in Mexico. Back in Europe, Humboldt visited further collections and published the detected hieroglyphic writings altogether with cultural objects and landscapes in the book `Vues des Cordillères et Monuments des Peuples Indigènes de l`Amerique, voyage de Humboldt et Bonpland´, labelled corresponding to the cultural background.
By scientific and culture historical analyses, the Humboldt codices are revised and related to each other and others. In especial, the compilation of fragments shown on plate 36 in the book is looked at more closely. Whereas most of the plates represent only one sheet of painted amate paper, here segments with details of seven fragments are put together. It is tried to comprehend why these pieces are on one plate.
To find out a common feature of the documents, their content and represented form are compared. A correlation between some pieces is obvious and thus is also expected in the manufacture of the codices, in the kind of material used. For this the inks and colors are determined by scientific analysis including XRF-, Raman-, FTIR- and VIS- spectroscopy. Special material is detected and related to results of former analysis of codices written during the colonial period of America. Herewith a clear cultural assignment of the manuscripts is performed.
A relation of the fragments represented on plate 36 among each other and to other codices of the collection Manuscripta Americana in Berlin is discussed. Also, if the manuscripts are unique `originals´ or represent fragments of documents, whose corresponding pieces maybe found- in the best case- incorporated in other collections. We detected, that at least two of them can be put into relation to similar manuscripts deposited in Mexico. Further material analysis should clarify, if the corresponding pieces are identical- from one document, or if one of them is a copy. Herewith an approximation to authenticity features and history is issued.
Hydrogenated nitrile butadiene rubber (HNBR) elastomer was thermo-oxidatively aged at different temperatures up to 150°C. Fourier transform infrared spectroscopy (FTIR), compression stress relaxation (CSR) and IRHD microhardness were used to characterise the chemo-mechanical changes of HNBR O-rings during thermo-oxidative ageing. FTIR shows the development of carbonyl, methyl and ester groups but the nitrile content was not affected by ageing. The effect of sample geometry during CSR was investigated. CSR data were converted through integrated kinetic laws. The conversion has proven its sensibility to detect heterogeneous ageing. This was confirmed by the IRHD measurements across the section of O-rings. Oxidation profiles were determined by applying the model of Wise et al. to the IRHD experimental results.
The site of Schöningen (Germany), dated to ca. 300,000 years ago, yielded the earliest large-scale record of humanly-made wooden tools. These include wooden spears and shorter double-pointed sticks, discovered in association with herbivores that were hunted and butchered along a lakeshore. Wooden tools have not been systematically analysed to the same standard as other Palaeolithic technologies, such as lithic or bone tools. Our multianalytical study includes micro-CT scanning, 3-dimensional microscopy, and Fourier transform infrared spectroscopy, supporting a systematic technological and taphonomic analysis, thus setting a new standard for wooden tool analysis. In illustrating the biography of one of Schöningen’s double-pointed sticks, we demonstrate new human behaviours for this time period, including sophisticated woodworking techniques. The hominins selected a spruce branch which they then debarked and shaped into an aerodynamic and ergonomic tool. They likely seasoned the wood to avoid cracking and warping. After a long period of use, it was probably lost while hunting, and was then rapidly buried in mud. Taphonomic alterations include damage from trampling, fungal attack, root damage and compression. Through our detailed analysis we show that Middle Pleistocene humans had a rich awareness of raw material properties, and possessed sophisticated woodworking skills. Alongside new detailed morphometrics of the object, an ethnographic review supports a primary function as a throwing stick for hunting, indicating potential hunting strategies and social contexts including for communal hunts involving children. The Schöningen throwing sticks may have been used to strategically disadvantage larger ungulates, potentially from distances of up to 30 metres. They also demonstrate that the hominins were technologically capable of capturing smaller fast prey and avian fauna, a behaviour evidenced at contemporaneous Middle Pleistocene archaeological sites.